X-shaped rigid methylthio arylethynes (MTA) have been demonstrated to mediate the assembly of gold nanoparticles. The structural attributes of MTAs include molecular rigidity, π-conjugation, and importantly the tunability in terms of size, shape, and binding strength. The size, kinetics, optical, and spectroscopic properties of the MTA mediated assembly are shown to be tunable by these structural attributes. This is the first example demonstrating an interparticle structurally tunable assembly in terms of size, shape, and binding properties, and an intriguing surface-enhanced Raman scattering effect as well. These findings could lead to unprecedented control of the interparticle spatial properties in nanoparticle assemblies for the exploitation of the unique optical and spectroscopic properties.

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